HRID1078357

反应详情

EQUATION

反应方程式

HRID 1078357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

3.5 g of 3-hydroxy-5-phenyl-isoxazole were dissolved in 100 ml of dimethylformamide. The solution was reacted with 3 g of finely powdered potassium carbonate and the reaction mixture was heated for 15 minutes at 100° C. in a nitrogen atmosphere. Then 5.8 g of 3-[N-(2-(3,4-dimethoxyphenyl)-ethyl)-N-methylamino]-propyl chloride were added batchwise. The reaction mixture was stirred for 4 hours at 100° C., after which the salts that formed were filtered off, the filtrate was concentrated to dryness, and the residue dissolved in methyl-tert-butyl ether. The solution was then washed with aqueous sodium carbonate solution, dried with magnesium sulfate, and concentrated to dryness. The remaining crude oily title compound that was left as a residue was purified by flash chromatography using ethyl acetate as the eluent. 4.75 g of the title compound were obtained.

WORKUP

后处理

  1. customafter which the salts that formed
  2. filtrationwere filtered off
  3. concentrationthe filtrate was concentrated to dryness
  4. dissolutionthe residue dissolved in methyl-tert-butyl ether
  5. washThe solution was then washed with aqueous sodium carbonate solution
  6. dry with materialdried with magnesium sulfate
  7. concentrationconcentrated to dryness
  8. waitThe remaining crude oily title compound that was left as a residue
  9. customwas purified by flash chromatography